Introduction: Salicylic acid is a derivative of benzoic acid and occurs in nature. The main target of this study was to develop the liquid chromatography coupled with tandem mass spectrometry technique as a method for determination of salicylic acid in feed materials and compound feed.
Material and Methods: Salicylic acid was extracted from feed with 0.1% hydrochloric acid in methanol. Separation was achieved in 8 min in a gradient elution using 0.1% formic acid and acetonitrile. The analyte was detected using negative electrospray tandem mass spectrometry. The procedure was validated to the specifications of the European Commission Decision No. 2002/657/EC.
Results: The validation results showed the repeatability of the method, which was evaluated at three levels (0.25, 0.5, and 1.0 mg/kg). Calibration curves for the working ranges were linear (R2 0.9911 to 0.9936), and recoveries ranged from 98.3% to 101%. The LOD and LOQ for compound feed were 0.02 and 0.05 mg/kg, respectively. Salicylic acid was found mostly in corn, and its concentrations differed depending on whether it was young or fully grown (5.30–12.8 mg/kg and 0.13–1.01 mg/kg, respectively).
Conclusions: A sensitive and reliable method for the determination of salicylic acid in feed and compound feed using LC-MS/MS was developed.
1. Armuła M.: Characteristics of salicylic acid and its effects in plants and animals. Nauki Przyrod 2014, 1, 10–37.
2. Clark I., Whitten R., Molyneux M., Taylor T.: Salicylates, nitric oxide, malaria, and Rey’s syndrome. Lancet 2001, 357, 625–627.
3. Commission Decision 2002/657/EC of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off J Eur Commun L 2002, 221, 8–36.
5. Gollapudi R.R., Teirstein P.S., Stevenson D.D., Simon R.A.: Aspirin sensitivity. Implication for patients with coronary artery disease. J Am Med Assoc 2004, 292, 3017–3023.
6. Kęszycka P.K., Szkop M., Gajewska D.: Overall content of salicylic acid and salicylates in food available on the European market. J Agric Food Chem 2017, 65, 11085–11091.
7. Olejnik M., Jedziniak P., Szprengier-Juszkiewicz T., Żmudzki J.: Influence of matrix effect on the performance of the method for the official control of non-steroidal anti-inflammatory drugs in animal muscle. Rapid Commun Mass Spectrom 2013, 27, 437–442.
8. Paterson J., Srivastava R., Baxter G., Graham A., Lawrence J.: Salicylic acid content of spices and its implication. J Agr Food Chem 2006, 54, 2891–2896.
9. Pietruk K., Olejnik M., Jedziniak P., Szprengier-Juszkiewicz T.: Determination of fifteen coccidiostats in feed at carry-over levels using liquid chromatography–mass spectrometry. J Pharm Biomed Anal 2015, 112, 50–59.
14. Scotter M.J., Roberts D.P.T., Wilson L.A., Howard F.A.C., Davis J., Mansell N.: Free salicylic acid and acetyl salicylic acid content of foods using gas chromatography-mass spectrometry. Food Chem 2007, 105, 273–279.
15. Swain A.R., Dutton S.P., Truswell A.S.: Salicylates in foods. J Am Diet Assoc 1985, 85, 950–960.
16. Szkop M., Szkop U., Gajewska D.: A simple and robust protocol for fast RP-HPLC determination of salicylates in foods. Food Anal Methods 2017, 10, 618–625.
17. Venema D.P., Hollman P.C.H., Janssen K.P.L.T.M., Katan M.B.: Determination of acetylsalicylic acid and salicylic acid in foods, using HPLC with fluorescence detection. J Agric Food Chem 1996, 44, 1762–1767.
18. Wood A., Baxter G., Thies F., Kyle J., Duthie G.: A systematic review of salicylates in foods: estimated daily intake of a Scottish population. Mol Nutr Food Res 2011, 55, 7–14.